US9067825B2 - Method for producing ternesite-belite calcium sulfoaluminate clinker - Google Patents

Method for producing ternesite-belite calcium sulfoaluminate clinker Download PDF

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US9067825B2
US9067825B2 US14/238,872 US201214238872A US9067825B2 US 9067825 B2 US9067825 B2 US 9067825B2 US 201214238872 A US201214238872 A US 201214238872A US 9067825 B2 US9067825 B2 US 9067825B2
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clinker
raw meal
period
phases
meal mixture
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US20140283712A1 (en
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Frank Bullerjahn
Dirk Schmitt
Mohsen Ben Haha
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Heidelberg Materials AG
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HeidelbergCement AG
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Priority claimed from EP20110006757 external-priority patent/EP2559674A1/de
Priority claimed from EP20120001488 external-priority patent/EP2636654A1/de
Priority claimed from EP20120002111 external-priority patent/EP2644577A1/de
Priority claimed from EP12002342.9A external-priority patent/EP2617691B1/de
Priority claimed from EP12003718.9A external-priority patent/EP2617692B1/de
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B7/00—Hydraulic cements
    • C04B7/345—Hydraulic cements not provided for in one of the groups C04B7/02 - C04B7/34
    • C04B7/3453—Belite cements, e.g. self-disintegrating cements based on dicalciumsilicate
    • C—CHEMISTRY; METALLURGY
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    • C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/02—Granular materials, e.g. microballoons
    • C04B14/04—Silica-rich materials; Silicates
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Definitions

  • the present invention relates to the production of a ternesite-belite-calcium sulfoaluminate (ferrite) clinker (TBC$A(F)).
  • the invention further relates to the use of alternative raw materials for clinker production, for example raw materials based on industrial byproducts, including those of low quality, such as lump slag and ash having a low glass content and/or a high free lime content and/or a high content of crystalline high-temperature phases, as well as naturally occurring rocks and rock glasses of comparative chemical composition.
  • calcium sulfoaluminate cement is normally produced by the sintering of homogenized, fine-particulate, natural raw materials, such as limestone, bauxite, gypsum/hemihydrate/anhydrite, aluminum-rich clay and an SiO 2 source, in a rotary kiln between 1100° C. and 1350° C. and has a significantly different chemism and phase content compared to Portland cement.
  • Table 1 compares the phases present in Portland cement (OPC) and sulfoaluminate cement (BC$AF).
  • Different industrial byproducts such as granulated blast furnace slag and fly ash, can also be added to the raw meal for sulfoaluminate cement.
  • a key, hydraulically active component of calcium sulfoaluminate cement is a (solid solution) crystal of the compounds of following composition 3CaO.3Al 2 O 3 .CaSO 4 .3CaO.3Fe 2 O 3 .CaSO 4 (C 4 A 3 $-C 4 F 3 $; sulfoaluminate-sulfoferrite, ye'elimite), which, once mixed with water and in the presence of soluble sulfates and additional calcium carriers, reacts to form ettringite, 3CaO.(Al 2 O 3 /Fe 2 O 3 ).3CaSO 4 .32H 2 O, as well as different monophases.
  • the (hydrate) phases formed can bind and permanently fix a large number of different (harmful) substances, for example by the incorporation into the crystal structure of the hydrate phase, agglomeration at particle surfaces, fixing in the cement lime, precipitation, for example as hydroxides/carbonates, and the like.
  • Two further hydraulically active phases of the calcium sulfoaluminate cement are dicalcium silicate (C 2 S) and tetracalcium-aluminate ferrite (C 4 AF), which primarily contribute to final strength, however.
  • EP 0 838 443 A1 describes the production of calcium sulfoaluminate cement on the basis of aluminum-containing residual materials.
  • FR 2 928 643 describes the production and composition of a belite-calcium sulfoaluminate (ferrite) clinker from a mixture comprising minerals which contain calcium, aluminum, silicon, iron and sulfur, preferably in the form of sulfate.
  • the raw meal mixture is sintered by being passed through a kiln with a pass-through time of at least 15 minutes.
  • These clinkers are mixed with hydraulic cement or cement of the Portland type to produce finished cement compositions.
  • the above object is thus solved by the production of a calcium sulfoaluminate clinker with the reactive C 5 S 2 $ phase as a main component, in which this phase is formed in larger amounts by optimizing the sintering of the raw meal composition according to the selected raw materials and the composition of the raw meal mixture.
  • the raw meal mixture is burned at least at 1200° C., preferably in the range of 1200° C. to 1350° C. and more preferably at 1250° C.
  • a specific step which differs significantly from the current prior art, is the subsequent selective tempering by controlling the temperature during a cooling phase in the kiln chamber as well as in the respective cooler system. Due to the selective temperature control during the cooling process, the burnt special clinker passes during cooling through a temperature range of 1200° C.
  • raw materials namely limestone, bauxites, aluminum-rich clays, sulfate carriers (anhydrite, gypsum and phosphogypsum) and calcium fluoride and/or raw materials having a high fluorine content, so as to obtain the desired reactive crystal Y phase.
  • fluorite, bauxite and aluminum-rich clays are very expensive raw materials and are only available in limited locations.
  • a potential solid solution crystal formation can also be established by determining the occupancy factors in a Rietveld refinement due to under-occupancies or mixed occupancies of individual atomic positions.
  • Another purely qualitative indicator is the change in color of the clinkers, which in some instances is significant.
  • the color of the clinkers which are subject to the two-stage method according to the invention thus changes, for example, from chestnut/ocher brown to green-brown all the way to a light gray hue.
  • Natural raw materials such as limestone, bauxite, clay/claystone, basalt, kimberlite, ingnimbrite, carbonatite, anhydrite, gypsum, etc. and/or industrial byproducts and residual materials, such as waste dump and landfill materials, ash and slag of both high and low quality, ceramic residues, sulfate plant muds and/or phosphogypsum are selected as sources for CaO, Al 2 O 3 (Fe 2 O 3 ), SiO 2 and SO 3 for the raw meal mixture.
  • Selected raw materials such as, for example but not exclusively, ashes
  • the secondary phases for example calcium silicates, sulfates, calcium aluminates, spinels, representatives of the melilite group, periclase, free lime, quartz and/or a glass phase, are preferably present in a proportion of 0.01 wt % to 30 wt %, preferably of 5 wt % to 20 wt % and more preferably of 10 wt % to 15 wt %.
  • the type and amount of one or more secondary phases in relation to the main components can be controlled by the ratios by weight of CaO/Al 2 O 3 ( ⁇ Fe 2 O 3 ), CaO/SiO 2 and by the proportion of the sulfate carrier in the raw meal mixture.
  • the contents of the main oxides of the clinker preferably comprise the following ranges:
  • the clinker according to the invention has a periclase content of >2 wt %.
  • the clinker may contain one or more secondary elements and/or compounds thereof from the group of the alkaline and alkaline earth metals and/or the transition metals and/or the metals and/or the semi-metals and/or the non-metals in a proportion of up to 20 wt %, preferably of ⁇ 15 wt % and more preferably of ⁇ 10 wt %.
  • concrete plasticizers and/or plasticizing admixtures are contained, preferably on the basis of ligninosulfonates, sulfonated naphthalene formaldehyde condensate, melamine formaldehyde condensate or phenol formaldehyde condensate, or on the basis of acrylic acid/acrylamide mixtures or polycarboxylate ethers, or on the basis of phosphated polycondensates.
  • a further advantage of the cement according to the invention or of the binder mixture produced therefrom is the formation of different phases during hydration (for example ettringite [AF t ], monophases [AF m ], metal-metal hydroxyl salts [LDH], etc.), which incorporate in their structure various heavy metals as well as other harmful substances (for example chlorides, etc.) and can thus permanently fix them.
  • phases during hydration for example ettringite [AF t ], monophases [AF m ], metal-metal hydroxyl salts [LDH], etc.
  • the invention also relates to all combinations of preferred embodiments, provided they are not mutually exclusive.
  • the expressions “around” or “approximately” mean that values that are higher or lower by at least 10% or values that are higher or lower by 5% and, in any case, values that are higher or lower by 1%, are included.
  • FIGS. 1 a and 1 b show the specific and cumulative heat flow of cement pastes M1 and M1a;
  • FIGS. 2 a and 2 b show the specific and cumulative heat flow of cement paste M2;
  • FIGS. 3 a and 3 b show the specific and cumulative heat flow of cement pastes L1, L1a and L1b;
  • FIGS. 4 a and 4 b show the specific and cumulative heat flow of cement pastes L2 and L2a;
  • FIGS. 5 a and 5 b show the specific and cumulative heat flow of cement pastes L3 and L3a;
  • FIG. 7 shows the specific heat flow of cement pastes from example 6.
  • Table 3 the raw materials used and with which the examples described hereinafter were carried out are characterized on the basis of the oxidic main components and degree of fineness thereof. The loss of weight after tempering at 1050° C. is also indicated. Table 4 shows the mineralogical phase composition of the industrial byproducts used.
  • the raw mixture consisted of 65 wt % (80% K1/20% MK)+5 wt % FA3+sulfate carrier and Al(OH) 3 . After sintering, the sample (M2) underwent the same cooling program as M1a and was then cooled.
  • the raw mixture consisted of 45 wt % K1+35 wt % S2+sulfate carrier and Al(OH) 3 .
  • a sample (L1) was cooled directly; the second sample (L1a) underwent the same cooling program as M1a after sintering and was then cooled; the third sample (L1b) underwent a cooling program after sintering in which the temperature was lowered from 1150° C. to 1100° C. over ⁇ 60 minutes, and the clinker was then cooled rapidly by exposure to air.
  • the raw mixture consisted of 37 wt % K1+54 wt % FA2+sulfate carrier and Al(OH) 3 . After sintering, a sample (L2) was cooled directly; the second sample (L2a) underwent the same cooling program as L1b after sintering and was then cooled.
  • the raw mixture consisted of 41 wt % K1+41 wt % S1+sulfate carrier and Al(OH) 3 . After sintering, a sample (L3) was cooled directly; the second sample (L3a) underwent the same cooling program as M1a after sintering and was then cooled.
  • the raw mixture consisted of 52.5 wt % CaCO 3 (Merck, analytical grade)+32.6 wt % FA2+MicroA and Al(OH) 3 .
  • two samples (CSAB1250_a and b) were cooled quickly and directly by exposure to air;
  • two further samples (CSAB1100_a and b) were cooled in the kiln to 1100° C. after sintering at 1250° C. and were kept at this temperature for 1 h and were then cooled quickly and directly by exposure to air.
  • the sulfate content of the raw meal was increased in two further samples (CSAB1100-SO3_a and b), then these samples underwent the same sintering and cooling program as CSAB1100_a and b.
  • Table 6 lists the lattice parameters and compositions determined for the clinkers obtained.
  • FIG. 6 shows the dependence of the lattice parameters on synthesis temperature and on the specific cooling program and on SO 3 content.
  • the clinker composition can be optimized and varied by optimizing the SO 3 /(Al 2 O 3 +Fe 2 O 3 ) ratios and by use of the specific production method (see Table 6).
  • the increasing incorporation of iron into the structure of ye'elimite correlates with the increase of the lattice parameters.
  • cubic modification instead of orthorhombic modification occurs during iron incorporation.
  • FIG. 7 shows the heat flow of hardened cement pastes formed from mixtures of 90% of the clinkers with 10% MicroA and of the pure clinker CSAB1100-SO3_b with a w/c value of 0.6.
  • Clinkers produced in accordance with the two-stage method according to the invention and having an optimized mineralogical composition clearly react/hydrate earlier. Experiments have shown that this is accompanied by a significant increase in early strength.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Combustion & Propulsion (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Civil Engineering (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Processing Of Solid Wastes (AREA)
  • Dispersion Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)
  • Glass Compositions (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Compounds Of Iron (AREA)
  • Lubricants (AREA)
  • Epoxy Resins (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Manufacture And Refinement Of Metals (AREA)
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EP11006757 2011-08-18
EP11006757.6 2011-08-18
EP20110006757 EP2559674A1 (de) 2011-08-18 2011-08-18 Ternesit-Belit-Calciumsulfoaluminat-Klinker und Verfahren zu seiner Herstellung
EP11008570 2011-10-26
EP11008570.1 2011-10-26
EP11008570 2011-10-26
EP12001488 2012-03-05
EP12001488.1 2012-03-05
EP20120001488 EP2636654A1 (de) 2012-03-05 2012-03-05 Ternesit als Additiv zu Calciumsulfoaluminatzement
EP12002111.8 2012-03-26
EP20120002111 EP2644577A1 (de) 2012-03-26 2012-03-26 Ternesit als Additiv zu Portlandzement
EP12002111 2012-03-26
EP12002342 2012-03-30
EP12002342.9 2012-03-30
EP12002342.9A EP2617691B1 (de) 2011-08-18 2012-03-30 Ternesit als Anreger für latent-hydraulische und puzzolanische Materialien
EP12003718 2012-05-10
EP12003718.9 2012-05-10
EP12003718.9A EP2617692B1 (de) 2011-08-18 2012-05-10 Verfahren und Additiv zur Steigerung der Frühfestigkeit und Verwendung des Additifs
PCT/EP2012/002978 WO2013023731A2 (de) 2011-08-18 2012-07-16 Verfahren zur herstellung von ternesit-belit-calciumsulfoaluminat-klinker

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